Method of obtaining stable aqueous emulsions of pitch and other unsaponified organic matter of mineral origin



Patented Dec. 20, 1927.

FRED CURTIS THORNLEY AND FRANK FORD TAI'PING, OF KNIGHTSBRIDGE, LONDON, AND OTTO BEYNARD, OF INKERMAN TERRACE, LONDON, ENGLAND, ASSIGNORS, BY DIRECT AND MESNE ASSIGNMENTS, TO THORNLEY AND COMPANY, A CORPORATION OF DELAWARE.

METHOD OF OBTAINING STABLE AQUEOUS EM'OLSIONS O1! PITCH AND OTB UNSAPONIFIED ORGANIC MATTER OF MINERAL ORIGIN.

No lilrawing. Application filed July 21, 192$,Serial No. 858,053, and in Great Britain January 26, 1928.

The subject of this invention is a method of obtaining stable aqueous emulsions of pitch and other unsaponified organic matter of mineral origin such as tar, coal tar pitch, petroleum pitch, or any pitch consisting mainly of carbon and hydrocarbons residues, also of insoluble hydrocarbons such as the higher members of the aromatic or paraflin series, including waxes.

According to this invention the said unsaponified matter either in the liquid or in a finely divided solid form is incorporated with a solution or pseudo-solution of an alginate together with cellulose in a state of colloidal fineness, and is heated to a suitable temperature with thorough agitation. The solution or suspension is heated to approximately its own boiling point, and the unsaponified matter added at any convenient temperature. During the agitation the mixture is maintained by continued external heating at ap-' proximately the boiling point of the mixture, the time required for carrying out the process being only that necessary for thorough mixture of the materials, not usually exceeding an hour. A stable emulsion is thereby produced, by virtue of the presence of the cellulose; such emulsion after cooling may be quite mobile and fluid, or thick and pasty, or semi-solid, or solid, according as the proportion of ingredients having a high melting point varies from a low percentage to a great preponderuncc.

Any water-soluble alginate may be used, for example, ammoniuni-alginate or sodiumalginate. An excess of ammonia or other alkaline material may be present at the beginning of the heating and agitation. The concentration of the alginate solution will be not less than one per cent and notmore than 10 per cent, The resulting products are true colloidal solutions, and it is possible to reverse the phases of the process and emulsify a small proportion of aqueous soluble alginate together with the cellulose (which ce'llulose is the structural part of the seaweed which is not removed during the preparation of the seaweed pulp, and which is in a very finely divided breless condition, in colloidal suspension) in a preponderating amount of tar, molten pitch,.or wax, the resulting liquid or solid emulsion also being stable.

The emulsions in which alginate solutions predominate. say for example an emulsion of 5 per cent of tar and 10 per cent of coal tar pitch or petroleum pitch in 85 'per cent of sodium alginate, or ammonium alginate solution and cellulose (in the proportions in which it is derived from the seaweed), are particularly suitable as binding agents for briquetting powdered coal or other fuel, as it is found that such binding agents c0mbine the properties of alginate'binders as regards structure and cohesion before and during combustion with the Water resisting properties of pitch.

Since the alginate is mixed with cellulose, it may be prepared from fresh seaweed by the following process:-

The seaweed, which may be Lmninarfa .s'fenoph-yllm, Lam-inarz'an digifata, Sargass'um baa-01' ferum. Lam-inmriacew maorocysf'z's, Laminarz'acem Nereocg stis Tuetkemno; or the like.

a is macerated or ground to a very fine state of division with or without a small proportion (say 1 per cent to 4 per cent) of water soluble alkaline material, such as anhydrous sodium carbonate, whereby a pulp is formed. This pulp may comprise cellulose suspended in a solution or jelly of a soluble a'lginate.

A preliminary maceration or pressing, with filtration, may in some cases be found desirable to evacuate the seawater mechanically entrained with the seaweed and the soluble salts contained therein. At any stage in the preparation of the pulp. a small amount of preservatives may be added, such as salicyclic acid or a salicylate, a phenol or a phenate, or other well-known material commonly employed to inhibit fermentation.

The fol owing are examples of the practical application of this invention Emample 1.

90 parts of 5% suspension of ammoniumalginate, together with 5 parts of cellulose ground to a state ofcolloidal fineness are placed in a stirring vessel and heated to nearly 100 degrees centigrade. Then 10 parts of heavy mineral oil in liquid form are gradually added and stirred in during a a mixture of tar and pitch.'

Any of the ingredients indicated by a, b or 0 above, mixed in any proportions with powdered naphthalene or with powdered or molten coal-tar pitch.

Example To 1 ton of finely divided seaweed pulp (of the nature already described) is added -100 lbs. of commercial ammonia liquor (containing 20 per cent ammonia) and after stir-' ring in the .ammonia liquor the pulp is heated nearly to boiling point. From 100 lbs. of heavy mineral oil such as fuel oil or t ransoil is then added to start the emulsi fication. A molten mixture consisting of 1750 lbs. of hard petroleum pitch or bitumen and 250 lbs. of fuel oil or similar heavy mineral oil maintained at temperature of 140-170 C. is then delivered on or into the pulp mixture with continuous stirring. A violent ebullition results, with consequent rapid evaporation, so that at the end of a period of from 30 to 60 minutes, when the action is complete, the resulting product may contain about 60 per cent of petroleum products and 40 per cent of ammonium alginate, cellulose, and water.

Ewample 3.

The ingredients and process are the same as in Example 2 above, and the proportions of said ingredients used are 280 lbs. pulp, 10 lbs. ammonia liquor, lbs. heavy mineral Example .4.

1 ton of coarsely crushed seaweed, which hasbeen drained and boiled to'eliminate its water-soluble contents, is mixed with 100 lbs. of commercial ammonia liquor. 1 ton of petroleum pitch, coal-tar pitch, or other solid bitumen-containing product, is roughly crushed to pass through a three-quarter inch mesh and added to the aforesaid ingredients.

The mixture of these three ingredients is now subjected to the intense grinding and incorporating action of a colloidal mill or similar device. To the resulting complex, which is solid in the cold state 5 per cent of'heavy mineral oil may now be added if desired to lower the meltingpoint of the final product. 1 The whole mixture is then heated with further agitation to a temperature of'140 to 170 C. until it is judged that emulsification is complete and a uniform product has been obtained.

What we claim and desire to secure by Letters Patent of the United States is A method of producing stable aqueous emulsions of unsaponified organic matter of mineral origin containing hydrocarbons, which consists in heating the said unsaponified organic matter to a temperature s'ufli:

ciently high to allow it to flow freely, and

then adding it rapidly with thorough agitation to a seaweed pulp comprising a hot colloidal aqueous suspension of cellulose in a water soluble alginate containing a water soluble alkaline aqueous suspension is at a temperature near its boiling point. a

FRED CURTIS THORNLEY.

FRANK FORD TAPPING.

OTTO REYNARD.

compound, while said 

